反应详情

温度

70 °C

To a solution of 5 g 2-(4-chloro-phenyl)-3-cyclopropylmethoxy-pyridine in 15 mL acetic acid, 3 mL hydrogenperoxyde (30% in water) was added. The reaction mixture was then stirred at 70° C. for 15 h. The reaction mixture was diluted with water and quenched with sodium carbonate. The mixture was washed with methylene chloride. The organic phase was washed with water; then dried over MgSO4 and purified by chromatography on silica gel with a gradient of ethyl acetate to ethyl acetate:methanol 4:1 to yield 3.46 g (65.19%) of the title compound as white solid, MS 276.1 (M+H)+.

1. customquenched with sodium carbonate
2. washThe mixture was washed with methylene chloride
3. washThe organic phase was washed with water
4. dry with materialthen dried over MgSO4
5. custompurified by chromatography on silica gel with a gradient of ethyl acetate to ethyl acetate:methanol 4:1